CN103267746A - Integrated laser probe component analyzer for macroscopic and micro-area component analysis - Google Patents
Integrated laser probe component analyzer for macroscopic and micro-area component analysis Download PDFInfo
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- CN103267746A CN103267746A CN2013101418941A CN201310141894A CN103267746A CN 103267746 A CN103267746 A CN 103267746A CN 2013101418941 A CN2013101418941 A CN 2013101418941A CN 201310141894 A CN201310141894 A CN 201310141894A CN 103267746 A CN103267746 A CN 103267746A
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Abstract
The invention belongs to the technical field of laser precision detection and discloses an integrated laser probe component analyzer for macroscopic and micro-area component analysis. The integrated laser probe component analyzer comprises a laser, a frequency multiplication module, two cage-type cubes, two laser wavelength reflectors, an industrial camera, a spectrum collector, an object lens converter, a focusing object lens, a spectrometer and a computer. A front end of a light outlet of the laser is provided with the frequency multiplication module. The laser is in an electric signal communication relationship with the computer. The integrated laser probe component analyzer can realize accurate qualitative analysis and high-precision quantitative analysis of macroscopic and micro-area components, can realize fast seamless switching of macroscopic and micro-area component analysis, has a modularization design and a compact structure, and improves an equipment integrated level. All the modules have independent functions and can be operated and maintained easily. Through the optical path modularization design, users can conveniently carry out optical path calibration before use so that operation time is saved and an analysis precision is improved.
Description
Technical field
The invention belongs to laser accurate detection technique field, be specially a kind of macroscopic view and microcell integrated laser probe analytical instrument, be mainly used in macroscopic view and the accurate qualitative analysis of microcell elemental composition and the quantitative test of degree of precision of material.
Background technology
Constituent analysis is engineering and material science research and the key means of producing.Laser-induced Breakdown Spectroscopy is analyzed (Laser-Induced breakdown Spectroscopy, be called for short LIBS) be to adopt the high-energy-density laser pulse to excite analyte, produce plasma, the atom of article on plasma body and the energy level transition characteristic spectrum of ion are analyzed simultaneously, draw the method for each element kind and content.Current, the subject matter that the laser probe technology exists is that interference and the matrix effect of other elements is big, and detection limit is relatively poor, is generally the per mille order of magnitude; Add used laser beam spot diameter big (50-100um), the bombardment degree of depth dark (10um) is so mainly be confined to macroscopical constituent analysis.In recent years, MicroLIBS rises, but the minimum light spot diameter also can only reach 10um.Therefore, the main trend of LIBS technical development at present is: the one, increase substantially detection limit and analysis precision; The 2nd, can be fit to the analysis of microstructure micro-area composition.
Chinese patent literature " a kind of component analyzer for laser probe micro-area " (bulletin is CN201434840, and the day for announcing is on March 31st, 2010) discloses a kind of component analyzer for laser probe micro-area.Its structure is: laser instrument, beam expanding lens and completely reflecting mirror are positioned on the same horizontal optical path successively; The reflecting surface of completely reflecting mirror and the angle of horizontal optical path are 45 degree; Industrial CCD is positioned at the top of completely reflecting mirror, and industrial CCD and first focusing objective len are placed and optical axis coincidence from top to bottom successively; The work top of three-dimensional working platform is positioned at the below of first focusing objective len; Completely reflecting mirror is movably arranged on the reflected light path of sample, and fibre-optical probe is positioned on the reflected light path of completely reflecting mirror; Industrial CCD is connected with the computing machine that has display by optical fiber, and fibre-optical probe is connected with grating spectrograph, enhancement mode CCD and computing machine.This laser probe instrument can carry out lossless detection to material microcell element, can satisfy the quick elemental composition qualitative analysis of the device of various materials and size, can also carry out quantitative test at trace even the trace element of sample microcell.
Chinese patent literature " a kind of component analyzer for laser probe micro-area based on double laser light source " (bulletin is CN101782517A, and the day for announcing is on July 21st, 2010) has been announced a kind of component analyzer for laser probe micro-area based on double laser light source.It is characterized in that: the light-emitting window of laser with fixed wavelength, attenuator, beam expanding lens, aperture, first semi-transparent semi-reflecting lens are positioned on the same horizontal optical path successively; First total reflective mirror is movable to be installed, parallel with first semi-transparent semi-reflecting lens when it is positioned at light path; Focusing objective len is positioned on the reflected light path of first completely reflecting mirror; Second semi-transparent semi-reflecting lens is between first completely reflecting mirror and focusing objective len, perhaps between first completely reflecting mirror and first semi-transparent semi-reflecting lens; Be placed with second total reflective mirror on the emitting light path of Wavelength tunable laser, the reflecting surface of second total reflective mirror and the angle of horizontal optical path are 45 degree, and first semi-transparent semi-reflecting lens is parallel with second total reflective mirror; Industrial CCD is fixed on support bracket fastened top, and is positioned at the top of first completely reflecting mirror, and industrial CCD is connected with computing machine by cable; Support bracket fastened below is traversing carriage, and the bottom of traversing carriage is equipped with the lens bracket rotating disk, has a plurality of lens brackets on the lens bracket rotating disk, and a focusing objective len all is installed on each lens bracket, the enlargement ratio difference of each focusing objective len; The below of conglomeration camera lens is the two-dimemsional number controlled machine, and the two-dimemsional number controlled machine places on the base station; The side of traversing carriage is equipped with screw mandrel and guide rail, and screw mandrel is connected with motor with guide rail, and Electric Machine Control screw mandrel and guide rail drive traversing carriage and move up and down along the z axle, constitute x-y-z three-axis moving system jointly with the two-dimemsional number controlled machine; Fibre-optical probe is positioned on the reflected light path of second semi-transparent semi-reflecting lens, and is connected with grating spectrograph by optical fiber, and grating spectrograph is connected back access computing machine with enhancement mode CCD simultaneously; Laser with fixed wavelength, Wavelength tunable laser link to each other with the digital delay generator respectively, and the digital delay generator is connected with enhancement mode CCD.Can reach the purpose of the qualitative or quantitative test of laser probe micro-area composition.
Above technology is to utilize the component analyzer for laser probe micro-area of list or double laser light source to carry out the example that material element is analyzed.This laser probe instrument analysis precision height, analyzable minimum site size scope is little, can reach the purpose of qualitative analysis and the quantitative test of laser probe micro-area composition.But there is following some deficiency in this device.At first, this device can only be applied to the micro-area composition analysis of sample, and namely it can only be that the microcell of several micrometer ranges carries out more accurate qualitative and quantitative analysis at the sample surfaces diameter, and can not satisfy the user to the demand of macroscopical qualitative analysis of sample; Secondly, if the user needs respectively material to be carried out macroscopic view and micro-area composition analysis, then must use macroscopic view and micro-area composition analytical equipment respectively.The equipment that above patent documentation is mentioned can not be realized the purpose that macroscopic view and micro-area composition are analyzed simultaneously, and when needs macroscopic view and microcell detection, uses two laser probe equipment to analyze respectively and also do not meet economical and requirement efficiently; At last, optical element reusing degree height in this device, for example, catoptron both had been used for laser optical path and had played reflector laser, was used for the imaging observation light path simultaneously again, caused the optical system design complicated, be not easy to correction and the maintenance of light path system, increased instrument cost and equipment and used complexity.
Summary of the invention
The object of the present invention is to provide a kind of macroscopic view and microcell integrated laser probe analytical instrument, can realize laser probe macroscopic view and the accurate qualitative analysis of micro-area composition and the quantitative test of degree of precision simultaneously.
A kind of macroscopic view provided by the invention and microcell integrated laser probe analytical instrument comprise laser instrument, times frequency module, first cage cube, the first optical maser wavelength catoptron, industrial camera, the second optical maser wavelength catoptron, second cage cube, spectra collection device, Nosepiece, focusing objective len, spectrometer and computing machine;
The front end of the light-emitting window of laser instrument is equipped with a times frequency module, and laser instrument and computer telecommunication number link to each other;
First cage cube and second cage cube are cube structure, and all have through hole on each face; The first optical maser wavelength catoptron drawing out type is installed in first cage cube; The second optical maser wavelength catoptron detachably is installed in second cage cube; The laser beam angle of the reflecting surface of the first optical maser wavelength catoptron and laser instrument emission is 45 degree; The second optical maser wavelength catoptron is positioned on the reflected light path of the first optical maser wavelength catoptron, and the angle of the reflecting surface of the second optical maser wavelength catoptron and the laser beam after the first optical maser wavelength mirror reflects is 45 degree;
First cage cube and second cage cube connect into an integral body by connecting link;
Nosepiece is between second cage cube and two-dimentional mobile platform, and two-dimentional mobile platform is used for placing sample; Have four rotatable laser focusing objective len interfaces on the Nosepiece at least, laser focusing objective len interface be used for to be installed the focusing objective len of different wave length and different focal, and Nosepiece cube links together by web member and second cage;
The spectra collection device be used for to be gathered laser beam ablation sample surfaces material and is formed the plasma flame signal, and the spectra collection device is connected with the spectrometer light signal, and spectrometer and computer telecommunication number link to each other;
Industrial camera be used for to be gathered the visible light signal of laser beam ablation sample surfaces material back reflection, and industrial camera and computer telecommunication number are connected.
Because the various shortcoming that existing LIBS equipment exists the invention provides technique scheme, can realize the purpose of the quantitative test of the accurate qualitative analysis of laser probe macroscopic view and micro-area composition and degree of precision simultaneously.Particularly, the present invention has following technical characterstic:
(1) the most outstanding technical characterstic of the present invention is to realize macroscopic view and micro-area composition analysis simultaneously.When the user needs to carry out macroscopical constituent analysis to material earlier, and then material carried out micro-area composition when analyzing, can macroscopical focusing objective len be placed on the 3rd optical axis by Nosepiece.Macroscopical focusing objective len has bigger focal length (being generally 100-200mm) among the present invention, the laser of Nd:YAG pulsed laser output can be focused on tens to the hundreds of micron, thereby realizes the purpose of the macroanalysis of material; After finishing macroanalysis, can switch to the microcosmic focusing objective len fast by the rotation Nosepiece, to have the characteristics of short focal length, large-numerical aperture (be that the microcosmic focus lamp of 532nm is example to focus on wavelength to the microcosmic focusing objective len among the present invention, its: f=10mm, N.A.=0.4), this microcosmic focusing objective len can be that the laser beam of 532nm focuses on the hot spot that diameter is 2.6um with wavelength, has approached the diffraction limit of this microcosmic focusing objective len.Thereby realize the purpose to the quantitative test of the accurate qualitative analysis of material micro-area composition and degree of precision.Among the present invention, the rotation by Nosepiece can realize the quick switching of macroscopic view and the constituent analysis of microcell laser probe, and macroscopic view and microcosmic laser probe analytical instrument are organically combined, and has realized that the height of two kinds of distinct devices is integrated.This macroscopic view and microcell integrated laser probe analytical instrument have that switch speed is fast, alignment precision is high, need not to recalibrate advantages such as light path and easy operating.
(2) another outstanding technical characterstic of the present invention is to have realized " coaxial collection " and " same shaft monitoring " simultaneously.At first, behind the plasma that laser excitation goes out, from coaxial light path, gather spectral signal, and transfer signals to the grating spectrograph of being furnished with ICCD by silica fibre, then send into calculating and processing that computing machine is correlated with, finally demonstrate intensity and the distribution situation of spectrum at terminal display.Secondly, another characteristics of this integrated laser probe analytical instrument can be carried out same shaft monitoring to the tissue regions of analyzing exactly when carrying out " coaxial collection ".In order to reach the purpose of " What You See Is What You Get ", the present invention has adopted coaxial monitoring system, the transmission light path that is laser beam is coaxial with imaging optical path, share mirror elements in the light path system to the influence on the light path system image quality in order to reduce, the catoptron (metal film plane mirror) that independently is used for imaging is housed with the shaft monitoring light path, its effect is with visible light path turnover 90 degree, visible light is reflexed on the imaging target surface of industrial CCD.In order not influence the carrying out of coaxial collection, this catoptron is fixed on the push-and-pull motor, and when needs carried out with shaft monitoring, this catoptron was pushed into specified location with it under the driving of push-and-pull motor; And observation is pulled away from second optical axis by the push-and-pull motor with catoptron when needing to gather spectrum after finishing.In addition, by the light path calibration, on the basis of shaft monitoring, can realize that the component lines in the big zone of an area scans and the scanning of composition face.
(3) complicated at the design of in the past LIBS equipment light path system, optical element quantity is many, the light path calibration difficulties, be not easy to a series of shortcomings such as later maintenance, the present invention adopts modular design method, laser mirror, laser focusing objective len, spectra collection head, industrial CCD are placed different standalone modules, by framed structure each separation module is fixed up.Modular design makes this equipment have that compact conformation, light path are easy to calibration, module is changed quick and safeguard advantages such as simple, and having strengthened greatly should macroscopic view and the integrated level of microcell integrated laser probe analytical instrument.
(4) in traditional LIBS equipment, change catoptron and focusing objective len and be extremely complexity and the process of poor efficiency, usually need just can finish for a long time replacing and the light path calibration of optical element, therefore, its laser mirror and focusing objective len are all at a certain specific wavelength design.And in the application of reality, usually need to adopt the dissimilar sample of different wavelength of laser pulse output ablation, the present invention has adopted the Nd:YAG pulsed laser (wavelength is respectively 266nm, 355nm, 532nm and 1064nm) with four kinds of different wave length outputs, in order to realize the quick switching of different optical maser wavelength outputs, designed special catoptron interface adapter and realized quick light path conversion.This interface adapter is the circular bottom plate that has draw-in groove, when needs are changed catoptron, the circular mirror holder that this optical maser wavelength catoptron is housed is inserted into the draw-in groove of circular bottom plate and rotates to the fixed position, namely finishes the replacing of catoptron.Then, open indication laser, can finely tune the inclination angle of catoptron easily and fast by three angle vernier adjustment knobs on this base, make the angle of catoptron and optical axis accurately be adjusted into 45 degree.
In sum, compare with present LIBS equipment, " macroscopic view and microcell integrated laser probe analytical instrument " has following technical advantage:
The first, can realize that " macroscopic view and microcell laser probe instrument " is integrated in same equipment, and can realize seamless quick switching; The second, can realize " coaxial collection " and " same shaft monitoring " simultaneously; The 3rd, modular design, compact conformation, device integration are higher; The 4th, laser focusing objective len and laser mirror (266/355/532/1064nm) replacing speed is fast, light path calibration simple and fast, and easy to operate, precision is higher;
" macroscopic view and microcell integrated laser probe analytical instrument " alternative existing independently macroscopic view or microcell laser probe analytical instrument, it not only can carry out the qualitative analysis of material macroscopic view composition, and can carry out the accurate qualitative analysis of material micro-area composition and the quantitative test of degree of precision, can be applied to numerous areas such as Materials Science and Engineering, machine-building, metallurgy, petrochemical complex, bioengineering, electronic engineering, nuclear physics, agricultural and safety detection.
Description of drawings
Fig. 1 is the three-dimensional structure synoptic diagram of first kind of embodiment of laser probe analytical instrument provided by the invention;
Fig. 2 is the three-dimensional structure synoptic diagram of second kind of embodiment of component analyzer for laser probe micro-area provided by the invention;
Fig. 3 is the three-dimensional structure synoptic diagram of the third embodiment of component analyzer for laser probe micro-area of the present invention;
Wherein, 1. laser instrument; 2. frequency module doubly; 3. cage cube; 4. circular adjustable cage base plate; 5. optical maser wavelength catoptron; 6. industrial camera; 7. long fulcrum bar; 8. sliding electromagnet; 9. circular adjustable cage base plate; 10. optical maser wavelength catoptron; 11. visible wavelength catoptron; 12. cage cube; 13. spectra collection device; 14. short strut; 15. location-plate; 16. Nosepiece; 17. laser focusing objective len; 18. two-dimentional mobile platform; 19. marble platform; 20. optical table; 21.X shaft step motor; 22.Y shaft step motor; 23. spectrometer; 24. display; 25. computing machine; 26. common worktable; 27. optical patchcord; 28. twisted-pair feeder; 29. kilomega network netting twine; 30. twisted-pair feeder; 31. concentric cable; 32. concentric cable; 33. the center has the broadband mirrors of light hole.
Embodiment
Below in conjunction with accompanying drawing the specific embodiment of the present invention is described further.Need to prove at this, understand the present invention for the explanation of these embodiments for helping, but do not constitute limitation of the invention.In addition, below in each embodiment of described the present invention involved technical characterictic just can not make up mutually as long as constitute conflict each other.
Can be used for laser probe, constituent analysis and same shaft monitoring according to this macroscopic view and microcell integrated laser probe analytical instrument.Analyser can be divided into three parts by function with it: (1) laser probe; (2) analytical instrument; (3) coaxial monitoring system.
Among the present invention, what laser instrument 1 adopted is the Nd:YAG pulsed laser, by the laser output that times frequency module 2 can obtain 266nm, 355nm, 532nm or four kinds of wavelength of 1064nm is installed at the front end of its light-emitting window.And laser instrument 1 links to each other with computing machine 25 by concentric cable 32, can realize whether directly control laser instrument 1 by computing machine launches laser.After the beam direction of laser instrument 1 emission is served as reasons forward.
Optical maser wavelength catoptron 5, laser instrument 1 and doubly frequency module 2 on same straight line.And optical maser wavelength catoptron 5 is 45 degree with the laser beam angle of laser instrument 1 emission, is used for laser beam turnover 90 degree with laser instrument 1 emission, and the laser beam exit direction after the turnover is for from right to left.Cage cubes 3 is cube structure, all has manhole on its 6 faces; And the size of the first optical maser wavelength catoptron 5 is less than the size of through hole on first cage cubes 3; Optical maser wavelength catoptron 5 is fixed on the circular adjustable cage base plate 4, the circular adjustable cage base plate 4 that optical maser wavelength catoptron 5 is housed is inserted in the top through hole of cage cubes 3, can regulate the angle of the laser beam of optical maser wavelength catoptron 5 and laser instrument 1 emission by reversing circular adjustable cage base plate 4, when angle is 45 when spending, can be with adjustable cage base plate 4 lockings by the trip bolt that screws on the cage cubes 3.
Optical maser wavelength catoptron 10 is positioned on the reflected light path of optical maser wavelength catoptron 5, and the angle of optical maser wavelength catoptron 10 and laser beam after 5 reflections of optical maser wavelength catoptron is 45 degree, is used for optical maser wavelength catoptron 5 laser light reflected Shu Zaici turnover 90 degree.Via the exit direction of the laser beam after optical maser wavelength catoptron 10 reflection for from top to bottom.Cage cubes 12 is identical with cage cube 3 structures; Optical maser wavelength catoptron 10 is fixed on the circular adjustable cage base plate 9, the size of the second optical maser wavelength catoptron 10 is less than the size of through hole on second cage cubes 12, the circular adjustable cage base plate 9 that optical maser wavelength catoptron 10 is housed is inserted in the anterior through hole of cage cubes 12, can regulate optical maser wavelength catoptron 10 and angle via the laser beam after 5 reflections of optical maser wavelength catoptron by reversing circular adjustable cage base plate 9, when angle is 45 when spending, can be with adjustable cage base plate 9 lockings by the trip bolt that screws on the cage cubes 12.
Wherein, cage cubes 3 and cage cubes 12 also is located along the same line, and cage cubes 12 is positioned at the left side of cage cubes 3, by four long fulcrum bars 7 cage cubes 3 and cage cubes 12 coupled together, and constitutes an integral body.
Location-plate 15, Nosepiece 16 and focusing objective len 17 are positioned at the below of cage cubes 12 from top to bottom successively, and all are located on the same line.Four laser focusing objective len interfaces are arranged on the Nosepiece 16, the focusing objective len 17 of four different wave lengths, different focal just is fixed on four laser focusing objective len interfaces of Nosepiece 16, and Nosepiece 16 and location-plate 15 link together by hickey simultaneously.Location-plate 15 links together by four short struts 14 and cage cubes 12, thereby cage cubes 12, location-plate 15, Nosepiece 16 and focusing objective len 17 are constituted an integral body.
According to above description, laser instrument 1, times frequency module 2, cage cubes 3, circular adjustable cage base plate 4, optical maser wavelength catoptron 5, long fulcrum bar 7, circular adjustable cage base plate 9, optical maser wavelength catoptron 10, cage cubes 12, short strut 14, location-plate 15, Nosepiece 16, laser focusing objective len 17, computing machine 25 and concentric cable 32 have just constituted the laser probe part of macroscopic view with microcell integrated laser probe analytical instrument.
According to above description, spectra collection device 13, optical patchcord 27, spectrometer 23, concentric cable 31, computing machine 25 and display 24 have just constituted the analytical instrument part of macroscopic view with microcell integrated laser probe analytical instrument.
Industrial camera 6 is positioned at the right side of cage cubes 3, and both are on same the straight line, and the right lateral surface of the central axis of industrial camera 6 and cage cubes 3 should keep vertical, thereby realizes the high-precision coaxial monitoring.Industrial camera 6 afterbodys are connected with kilomega network netting twine 29, and the other end of kilomega network netting twine 29 links to each other with computing machine 25.Sliding electromagnet 8 is positioned at the rear of cage cubes 12, and both are on the same straight line, and the rear surface of the central axis of sliding electromagnet and cage cube is vertical, and sliding electromagnet 8 links to each other with computing machine 25 by twisted-pair feeder 28.Fixedly there is visible wavelength catoptron 11 on the removable axis top of sliding electromagnet 8, visible wavelength catoptron 11 is positioned at cage cubes 12, be positioned at simultaneously optical maser wavelength catoptron 10 under, and the reflecting surface of the reflecting surface of visible wavelength catoptron 11 and optical maser wavelength catoptron 10 is parallel to each other, and namely the angle of visible optical wavelength catoptron 11 and the laser beam after 5 reflections of optical maser wavelength catoptron is 45 degree.By the control to sliding electromagnet, can realize the lower horizontal of visible wavelength catoptron 11 from optical maser wavelength catoptron 10 shifted out and move into, be about to shifting out and moving into cage cubes 12 of visible wavelength catoptron 11 front and back, level.
According to above description, industrial camera 6, sliding electromagnet 8, visible wavelength catoptron 11, twisted-pair feeder 28, kilomega network netting twine 29 and computing machine 25 have just constituted the coaxial monitoring system of macroscopic view with microcell integrated laser probe analytical instrument.
In addition, this macroscopic view and microcell integrated laser probe analytical instrument also comprise some auxiliary devices except above three major parts.Specifically describe as follows: two-dimentional mobile platform 18 be positioned at laser focusing objective len 17 under, and two-dimentional mobile platform 18 is positioned at the top of marble platform 19, and uses screw that two-dimentional mobile platform 18 is fixing with marble platform 19.The two dimension mobile platform is realized moving horizontally of X and Y-axis by X-axis stepper motor 21 and y-axis stepper motor 22, and X-axis stepper motor 21 links to each other with computing machine 25 by twisted-pair feeder 30 with y-axis stepper motor 22 and realizes the mobile control of X and Y-axis; Optical table 20 is used for placing and fixed laser 1 and times frequency module 2; Common worktable 26 is used for placing spectrometer 23, computing machine 25 and display 24.
What deserves to be explained is computing machine 25 inner simultaneously integrated laser instrument control software, spectral component analysis software, coaxial Monitoring and Controlling software, magnet control software, displacement platform control software.Though every software mentioned above all has the ripe supporting use of business software, but consider that the present invention is convenient to use demand to requirement and the user of software integrated level to software operation, the present invention adopts C/C++ language and MFC (Microsoft Foundation Classes: the basis of software class libraries) write a cover and had the integrated control software systems of Windows interfacial characteristics, realize the purpose of the multiple control in interface, namely under this software operation interface, can realize laser probe simultaneously, constituent analysis, with every functions such as shaft monitoring and two dimensional motions.
The present invention also can adopt the structure shown in the accompanying drawing 2, and it is that with the key distinction of the macroscopic view shown in the accompanying drawing 1 and microcell integrated laser probe analytical instrument the locus of coaxial monitoring system is different.Be specially visible wavelength catoptron 11 vertically mobile until shifting out cage cubes 12 downwards, make visible wavelength catoptron 11 between cage cubes 12 and location-plate 15, and the reflecting surface of the reflecting surface of maintenance visible wavelength catoptron 11 and optical maser wavelength catoptron 10 is parallel to each other, and namely the angle of visible optical wavelength catoptron 11 and the laser beam after 5 reflections of optical maser wavelength catoptron is 45 degree.Meanwhile industrial camera 6 is moved on to the below on the right side, cage cubes 3 of visible wavelength catoptron 11, and the angle of the reflecting surface of the central axis of industrial camera 6 and visible wavelength catoptron 11 is 45 degree, thereby guarantees can vertically inject in the industrial camera 6 through the visible light of visible wavelength catoptron 11 reflections.Identical in the locus of remaining part and the accompanying drawing 1.
In addition for simplified structure, we can also adopt the structure shown in the accompanying drawing 3, version in this structure and the accompanying drawing 2 is similar, difference is that this macroscopic view and microcell integrated laser probe analytical instrument have removed sliding electromagnet 8 and twisted-pair feeder 28, visible wavelength catoptron 11 centers of being replaced by have the broadband mirrors 33 of light hole, and (purpose that the center has a light hole is that to make spectral range be that the visible light of 400nm～700nm can pass through this catoptron, be that visible light passes from light hole, thereby do not influence coaxial gatherer process), the spectral reflectance bandwidth (being the spectrum of reflected light scope) that the center has the broadband mirrors 33 of light hole is 200nm～1000nm.Industrial camera 6 and spectra collection device 13 transpositions.The locus of each parts and angular relationship are: the broadband mirrors 33 that the center has a light hole is between cage cubes 12 and location-plate 15, and to have a reflecting surface of the reflecting surface of broadband mirrors 33 of light hole and optical maser wavelength catoptron 10 parallel to each other at the maintenance center, the angle that is the laser beam after the center has the broadband mirrors 33 of light hole and reflects through optical maser wavelength catoptron 5 is 45 degree (purpose is transmission direction turnover 90 degree with the spectral signal of incident, thereby the spectral signal process optical maser wavelength catoptron 10 back turnovers of transmission are straight up transmitted to the right for level).Spectra collection device 13 is positioned at the below on right side that the center has the broadband mirrors 33 of light hole, cage cubes 3, and the angle of reflecting surface that the central axis of spectra collection device 13 and center have the broadband mirrors 33 of light hole is 45 degree, thereby the broadband mirrors 33 spectrum of reflected light signals that have a light hole through the center can vertically be injected in the spectra collection device 13, guarantee alignment precision and the effect of coaxial collection; Industrial camera 6 be positioned at cage cubes 12 directly over and on same straight line, and the plane, top of the central axis of industrial camera 6 and cage cubes 12 keeps vertical, thereby realizes that high-precision coaxial monitors.Identical in the locus of remaining part and the accompanying drawing 1.
In this example, the spectral reflectance bandwidth of broadband mirrors 33 is that the spectrum of reflected light scope is 200nm～1000nm.The first optical maser wavelength catoptron 5, the second optical maser wavelength catoptron 10 are dichroic mirror, this dichroic mirror manufactures and designs at a certain specific wavelength laser output, be that it has high reflectivity to this wavelength laser bundle, and other wavelength laser or spectral signal are all had through characteristic.
Laser focusing objective len 17 adopts the micro-focusing objective len of large-numerical aperture, the glass material of this microcobjective is the ultraviolet fused quartz, glass surface is coated with anti-reflection film (realizing the high permeability to a certain specific wavelength laser beam), this micro-focusing objective len can focus on the laser beam of incident below the 3um, namely realizes the constituent analysis of microcell laser probe; Laser focusing objective len 17 can also adopt common focusing objective len (perhaps being called low numerical aperture focusing objective len) in addition, and this focusing objective len can focus on the laser beam of incident below the 100um, thereby realizes macroscopical laser probe constituent analysis.
The operating process of macroscopic view provided by the invention and microcell integrated laser probe analytical instrument is divided into macroscopical constituent analysis and micro-area composition is analyzed two kinds, and concrete operation steps is as follows:
At first be macroscopical constituent analysis:
1. preliminary work: at first, according to analyzing requirement, at the light-emitting window front end of laser instrument 1 times frequency module 2 is installed and is realized the purpose of a certain wavelength laser output (this laser instrument 1 can be realized the laser output of 266nm, 355nm, 532nm or four kinds of wavelength of 1064nm by times frequency module 2 is installed at its light-emitting window front end), this operation steps all is output as example with the 532nm wavelength laser; Secondly, change optical maser wavelength catoptron 5 and optical maser wavelength catoptron 10, two kinds of optical maser wavelength catoptrons all have higher reflectivity (reflectivity generally can reach more than 90%) to 532nm laser, simultaneously optical maser wavelength catoptron 5 and optical maser wavelength catoptron 10 are adjusted to definite angle, namely two catoptrons with towards the laser beam angle of incident separately be 45 degree; At last, rotation Nosepiece 16 uses the laser focusing objective len 17 (the laser focusing objective len that can carry out macroanalysis among the present invention can focus on the laser beam of 532nm diameter and be the laser facula below the 50um) that can carry out macroanalysis to realize changing laser focusing objective len 17.
2. sample preparation and placement: in order better sample to be carried out macroscopical constituent analysis, guarantee the precision of macroscopical constituent analysis, generally need earlier sample surfaces to be done polishing and the depth of parallelism and handle.The table top center that the sample of handling is placed into two-dimentional workbench gets final product;
3. same shaft monitoring: at first, by the control of computing machine 25 realizations to sliding electromagnet 8, drive signal for 8 one of sliding electromagnets, it is pushed into visible wavelength catoptron 11 in the cage cubes 12 by the manhole of cage cube 12 rear sides, be about to visible wavelength catoptron 11 place optical maser wavelength catoptron 10 under, and optical maser wavelength catoptron 10 is parallel to each other with the reflecting surface of visible wavelength catoptron.Meanwhile, drive industrial camera 6 by computing machine 25, after visible light process visible wavelength catoptron 11 reflections of sample surfaces emission, visible light just enters into industrial camera 6, open coaxial Monitoring and Controlling software this moment, will occur the picture with shaft monitoring on the screen of display 24.
In the structure shown in the accompanying drawing 3, because the broadband mirrors 33 of having removed sliding electromagnet 8 and visible wavelength catoptron 11 centers of being replaced by having been had light hole on the structure, and with industrial camera 6 place cage cubes 12 directly over, therefore when carrying out with shaft monitoring, only need drive industrial camera 6 by computing machine 25, enter into industrial camera 6 from the visible light of sample surfaces emission by the center pit that the center has the broadband mirrors 33 of light hole, meanwhile open coaxial Monitoring and Controlling software, the picture with shaft monitoring on the screen of display 24, will occur.
4. the control of two-dimensional stage: in the picture with shaft monitoring, we can see the sample location in space clearly.When certain a bit carries out a some constituent analysis on we need be to sample surfaces, monitoring picture by display 24 demonstrations, click and need the point analyzed on the sample surfaces, computing machine 25 can calculate the position and the X of monitoring picture center and the side-play amount of Y-direction that clicks automatically, after confirming that finishing the sample spot position chooses, computing machine 25 gives X-axis stepper motor 21 and y-axis stepper motor 22 to drive signal by twisted-pair feeder 30, finishes the shift action of two-dimentional mobile platform.
5. macroscopical constituent analysis: this step comprises two processes in fact, i.e. laser probe and macroscopical constituent analysis.But these two steps are almost carried out at the same time, and laser probe and constituent analysis are carried out synchro control by computing machine 25, introduce two processes below respectively.
A. laser probe: laser instrument 1 links to each other with computing machine 25 by concentric cable 32, realized the control of 25 pairs of laser instruments 1 of computing machine, at the front end of the light-emitting window of laser instrument 1 output (this introduction is output as example with 532nm optical maser wavelength) that times frequency module 2 has been realized a certain optical maser wavelength has been installed.At first, drive signal for 8 one of sliding electromagnets by computing machine 25, make it that visible wavelength catoptron 11 is shifted out cage cubes 12 by the manhole of cage cube 12 rear sides, be about to visible wavelength catoptron 11 and under optical maser wavelength catoptron 10, detach, meanwhile close industrial camera 6; Secondly, by the bright dipping of computing machine 25 control laser instruments 1, we can go out light frequency, bright dipping number of times and three parameters of single pulse energy by what computing machine 25 was controlled laser instrument 1.We are example with the monopulse analysis, namely utilize computing machine 25 control laser instruments 1 emission laser once, the laser beam of emission is successively by behind optical maser wavelength catoptron 5, optical maser wavelength catoptron 10 and the laser focusing objective len 17, laser beam is focused on the surface of sample by laser focusing objective len 17, the material of the laser spots ablation sample surfaces after the focusing (can be metal, nonmetal and stupalith) makes material ionization form plasma flame.More than the process of laser probe has just been finished in operation;
B. macroscopical constituent analysis: after laser instrument 1 emission laser beam, laser beam is passed through optical maser wavelength catoptron 5, optical maser wavelength catoptron 10 and laser focusing objective len 17 successively, laser beam is focused onto sample surfaces and forms laser focal beam spot (laser focal beam spot diameter is below 50um), thereby ablation sample surfaces material forms plasma flame.Plasma flame to around the space radiation plasma spectrometry, the plasma spectrometry in the numerical aperture of laser focusing objective len 17 only, can be by the lens combination of laser focusing objective len, and enter into spectra collection device 13 after seeing through optical maser wavelength catoptron 10 successively, spectra collection device 13 is sent to the plasma spectrometry that collects in the spectrometer 23 by optical patchcord 27, there are spectrum beam splitter and ICCD image-forming component in spectrometer inside, thereby separation and the imaging of the different spectral signals of article on plasma body spectrum kind (being the radiation of different wave length) have been realized, ICCD converts the plasma light spectrum signal that separates to electric signal by light signal, be sent in the computing machine 25 via concentric cable 31, computing machine 25 utilizes its inner integrated spectral component analysis software to carry out constituent analysis to spectral signal, provide the element term of a certain spectral signal correspondence, and show at the screen of display 24.
6. end analytic process: above step has namely been finished the whole operation process of macroscopical constituent analysis, enters into last step below, namely finishes analytic process.At first, by computing machine 25 control laser instruments 1, make its inside stop pump and just move (the Nd:YAG laser instrument is pulsed laser, and its inside has flashlamp that the Nd:YAG crystal is carried out pump Pu, thereby realizes laser pulse output), manual-lock laser power supply then; Secondly, by computing machine 25 control spectrometers 23, give 23 1 cooling signals of spectrometer, to the ICCD of spectrometer inside disposals of lowering the temperature, when treating that temperature is reduced to the temperature of technical requirement, get final product manual-lock spectrometer 23; Again, close industrial camera 6, and two-dimentional mobile platform 18 and sliding electromagnet 8 are resetted, above process is finished by computing machine 25 controls; At last, sample is shifted out from two-dimentional mobile platform 18, again the surface is polished and handle with the depth of parallelism in order to use when analyzing next time, after finishing dealing with, get final product in the storage cabinet that sample is placed.
We can also carry out constituent analysis to the microcell of sample, and detailed process is as follows:
1. preliminary work: at first, according to analyzing requirement, at the light-emitting window front end of laser instrument 1 times frequency module 2 is installed and is realized the purpose of a certain wavelength laser output (this laser instrument 1 can be realized the laser output of 266nm, 355nm, 532nm or four kinds of wavelength of 1064nm by times frequency module 2 is installed at its light-emitting window front end), this operation steps is output as example with the 532nm wavelength laser equally; Secondly, change optical maser wavelength catoptron 5 and optical maser wavelength catoptron 10, two kinds of optical maser wavelength catoptrons all have higher reflectivity (reflectivity generally can reach more than 90%) to 532nm laser, simultaneously optical maser wavelength catoptron 5 and optical maser wavelength catoptron 10 are adjusted to definite angle, namely two catoptrons with towards the laser beam angle of incident separately be 45 degree; At last, rotation Nosepiece 16 uses and can carry out the laser focusing objective len 17 (the laser focusing objective len 17 that carries out the micro-area composition analysis among the present invention can focus on the laser beam of 532nm diameter and be the laser facula below the 9um) that micro-area composition is analyzed to realize changing laser focusing objective len 17.
2. sample preparation and placement: in order better sample to be carried out the micro-area composition analysis, guarantee the precision that micro-area composition is analyzed, generally need earlier sample surfaces to be done polishing and the depth of parallelism and handle.The table top center that the sample of handling is placed into two-dimentional workbench gets final product;
3. same shaft monitoring: at first, by the control of computing machine 25 realizations to sliding electromagnet 8, drive signal for 8 one of sliding electromagnets, it is pushed into visible wavelength catoptron 11 in the cage cubes 12 by the manhole of cage cube 12 rear sides, be about to visible wavelength catoptron 11 place optical maser wavelength catoptron 10 under, and optical maser wavelength catoptron 10 is parallel to each other with the reflecting surface of visible wavelength catoptron.Meanwhile, drive industrial camera 6 by computing machine 25, after visible light process visible wavelength catoptron 11 reflections of sample surfaces emission, visible light just enters into industrial camera 6, open coaxial Monitoring and Controlling software this moment, will occur the picture with shaft monitoring on the screen of display 24.
In the structure shown in the accompanying drawing 3, because the broadband mirrors 33 of having removed sliding electromagnet 8 and visible wavelength catoptron 11 centers of being replaced by having been had light hole on the structure, and with industrial camera 6 place cage cubes 12 directly over, therefore when carrying out with shaft monitoring, only need drive industrial camera 6 by computing machine 25, enter into industrial camera 6 from the visible light of sample surfaces emission by the center pit that the center has the broadband mirrors 33 of light hole, meanwhile open coaxial Monitoring and Controlling software, the picture with shaft monitoring on the screen of display 24, will occur.
4. the control of two-dimensional stage: in the picture with shaft monitoring, we can see the pattern in sample microstructure zone clearly.When we need a bit carry out a some constituent analysis on the sample microstructure zone certain, monitoring picture by display 24 demonstrations, click and need the point analyzed on the sample surfaces, computing machine 25 can calculate the position and the X of monitoring picture center and the side-play amount of Y-direction that clicks automatically, after confirming that finishing the sample spot position chooses, computing machine 25 gives X-axis stepper motor 21 and y-axis stepper motor 22 to drive signal by twisted-pair feeder 30, finishes the action that the precision of two-dimentional mobile platform moves.
5. micro-area composition analysis: this step also comprises two processes, i.e. laser probe and micro-area composition analysis.But these two steps are almost carried out at the same time, and laser probe and constituent analysis are carried out synchro control by computing machine 25, introduce two processes below respectively.
A. laser probe: laser instrument 1 links to each other with computing machine 25 by concentric cable 32, realized the control of 25 pairs of laser instruments 1 of computing machine, at the front end of the light-emitting window of laser instrument 1 output (this introduction is output as example with 532nm optical maser wavelength) that times frequency module 2 has been realized a certain optical maser wavelength has been installed.At first, drive signal for 8 one of sliding electromagnets by computing machine 25, make it that visible wavelength catoptron 11 is shifted out cage cubes 12 by the manhole of cage cube 12 rear sides, be about to visible wavelength catoptron 11 and under optical maser wavelength catoptron 10, detach, meanwhile close industrial camera 6; Secondly, by the bright dipping of computing machine 25 control laser instruments 1, we can go out light frequency, bright dipping number of times and three parameters of single pulse energy by what computing machine 25 was controlled laser instrument 1.We are example with the monopulse analysis, namely utilize computing machine 25 control laser instruments 1 emission laser once, the laser beam of emission is successively by behind optical maser wavelength catoptron 5, optical maser wavelength catoptron 10 and the laser focusing objective len 17, laser beam is focused on the surface of sample by laser focusing objective len 17, the material of the laser spots ablation sample surfaces after the focusing (can be metal, nonmetal and stupalith) makes material ionization form plasma flame.More than the process of laser probe has just been finished in operation;
B. constituent analysis: after laser instrument 1 emission laser beam, laser beam is passed through optical maser wavelength catoptron 5, optical maser wavelength catoptron 10 and laser focusing objective len 17 successively, laser beam is focused onto sample surfaces and forms minimum laser focal beam spot (the focal beam spot diameter is that 9um is following), thereby ablation sample surfaces material forms plasma flame.Plasma flame to around the space radiation plasma spectrometry, the plasma spectrometry in the numerical aperture of laser focusing objective len 17 only, can be by the lens combination of laser focusing objective len, and enter into spectra collection device 13 after seeing through optical maser wavelength catoptron 10 successively, spectra collection device 13 is sent to the plasma spectrometry that collects in the spectrometer 23 by optical patchcord 27, there are spectrum beam splitter and ICCD image-forming component in spectrometer inside, thereby separation and the imaging of the different spectral signals of article on plasma body spectrum kind (being the radiation of different wave length) have been realized, ICCD converts the plasma light spectrum signal that separates to electric signal by light signal, be sent in the computing machine 25 via concentric cable 31, computing machine 25 utilizes its inner integrated spectral component analysis software to carry out constituent analysis to spectral signal, provide the element term of a certain spectral signal correspondence, the details of compositions such as the content in sample and ratio, and show at the screen of display 24.
6. end analytic process: above step has namely been finished the whole operation process of macroscopical constituent analysis, enters into last step below, namely finishes analytic process.At first, by computing machine 25 control laser instruments 1, make its inside stop pump and just move (the Nd:YAG laser instrument is pulsed laser, and its inside has flashlamp that the Nd:YAG crystal is carried out pump Pu, thereby realizes laser pulse output), manual-lock laser power supply then; Secondly, by computing machine 25 control spectrometers 23, give 23 1 cooling signals of spectrometer, to the ICCD of spectrometer inside disposals of lowering the temperature, when treating that temperature is reduced to the temperature of technical requirement, get final product manual-lock spectrometer 23; Again, close industrial camera 6, and two-dimentional mobile platform 18 and sliding electromagnet 8 are resetted, above process is finished by computing machine 25 controls.At last, sample is shifted out from two-dimentional mobile platform 18, again the surface is polished and handle with the depth of parallelism in order to use when analyzing next time, after finishing dealing with, get final product in the storage cabinet that sample is placed.
In a word, the present invention combines macroscopic view and microcell laser probe, can carry out the quantitative test of accurate qualitative analysis and degree of precision to macroscopic view and the micro-area composition of material, and can realize quick seamless switching between macroscopic view and micro-area composition analysis; Secondly, this equipment is modular design, and compact conformation has strengthened the integrated level of equipment.In addition, function independence, easy operating and maintenance between each module; At last, the modular design of light path makes the family conveniently use preceding calibration to light path, has saved the time, and simultaneously, analysis precision is higher.
The above is preferred embodiment of the present invention, but the present invention should not be confined to the disclosed content of this embodiment and accompanying drawing.So everyly do not break away from the equivalence of finishing under the spirit disclosed in this invention or revise, all fall into the scope of protection of the invention.
Claims (8)
1. a laser probe analytical instrument comprises laser instrument (1), times frequency module (2), first cage cube (3), the first optical maser wavelength catoptron (5), industrial camera (6), the second optical maser wavelength catoptron (10), second cage cube (12), spectra collection device (13), Nosepiece (16), focusing objective len (17), spectrometer (23) and computing machine (25);
The front end of the light-emitting window of laser instrument (1) is equipped with a times frequency module (2), and laser instrument (1) links to each other with computing machine (25) electric signal;
First cage cube (3) and second cage cube (12) are cube structure, and all have through hole on each face; First optical maser wavelength catoptron (5) drawing out type is installed in first cage cube (3); The second optical maser wavelength catoptron (10) detachably is installed in second cage cube (12); The laser beam angle of the reflecting surface of the first optical maser wavelength catoptron (5) and laser instrument (1) emission is 45 degree; The second optical maser wavelength catoptron (10) is positioned on the reflected light path of the first optical maser wavelength catoptron (5), and the angle of the reflecting surface of the second optical maser wavelength catoptron (10) and the laser beam after the reflection of the first optical maser wavelength catoptron (5) is 45 degree;
First cage cube (3) and second cage cube (12) connect into an integral body by connecting link;
Nosepiece (16) is positioned between second cage cube (1) and the two-dimentional mobile platform (18), and two-dimentional mobile platform (18) is used for placing sample; Have four rotatable laser focusing objective len interfaces on the Nosepiece (16) at least, laser focusing objective len interface is used for installing the focusing objective len (17) of different wave length and different focal, and Nosepiece (16) links together by web member and second cage cube (12);
Spectra collection device (13) is used for gathering laser beam ablation sample surfaces material and forms the plasma flame signal, and spectra collection device (13) is connected with spectrometer (23) light signal, and spectrometer (23) links to each other with computing machine (25) electric signal;
Industrial camera (6) is used for gathering the visible light signal of laser beam ablation sample surfaces material back reflection, and industrial camera (6) is connected with computing machine (25) electric signal.
2. laser probe analytical instrument according to claim 1, it is characterized in that, this analyser also comprises sliding electromagnet (8) and visible wavelength catoptron (11), visible wavelength catoptron (11) is installed on the sliding electromagnet (8), sliding electromagnet (8) moves in the cage cube (12) for drive visible wavelength catoptron (11) and is positioned at the second optical maser wavelength catoptron (10) below, and make the minute surface of the minute surface of visible wavelength catoptron (11) and optical maser wavelength catoptron (10) parallel to each other, the visible light signal of laser beam ablation sample surfaces material back reflection incides in the industrial camera (6) after by visible wavelength catoptron (11) reflection; Spectra collection device (13) is positioned at the top of first cage cube (3), and laser beam ablation sample surfaces material forms the plasma flame signal and is incident to spectra collection device (13) through the second optical maser wavelength catoptron (10).
3. laser probe analytical instrument according to claim 1, it is characterized in that, this analyser also comprise sliding electromagnet (8) and and visible wavelength catoptron (11), visible wavelength catoptron (11) is installed on the sliding electromagnet (8), sliding electromagnet (8) is used for driving visible wavelength catoptron (11) and moves between cage cube (12) and the location-plate (15), and make the minute surface of the minute surface of visible wavelength catoptron (11) and optical maser wavelength catoptron (10) parallel to each other, the visible light signal of laser beam ablation sample surfaces material back reflection incides in the industrial camera (6) after being reflected by visible wavelength catoptron (11), spectra collection device (13) is positioned at the top of first cage cube (3), and laser beam ablation sample surfaces material forms the plasma flame signal and is incident to spectra collection device (13) through the second optical maser wavelength catoptron (10).
4. laser probe analytical instrument according to claim 1, it is characterized in that, this analyser comprises that also the center has the broadband mirrors of light hole (33), broadband mirrors (33) is positioned between cage cube (12) and the location-plate (15), and the reflecting surface of broadband mirrors (33) and optical maser wavelength catoptron (10) is surperficial parallel to each other, industrial camera (6) is positioned at the top of cage cube (12), the visible light signal of laser beam ablation sample surfaces material back reflection is in light hole is incident to industrial camera (6), and laser beam ablation sample surfaces material incides spectra collection device (13) after forming the plasma flame signal has light hole by the center broadband mirrors (33) reflection.
5. according to arbitrary described laser probe analytical instrument in the claim 4, it is characterized in that the spectrum of reflected light scope of described broadband mirrors (33) is 200nm～1000nm.
6. according to arbitrary described laser probe analytical instrument in the claim 1 to 5, it is characterized in that times frequency module (2) is used for realizing the laser output of 266nm, 355nm, 532nm or four kinds of wavelength of 1064nm.
7. according to arbitrary described laser probe analytical instrument in the claim 1 to 5, it is characterized in that, the first optical maser wavelength catoptron (5) and the second optical maser wavelength catoptron (10) are dichroic mirror, this dichroic mirror only has high reflectivity to a certain wavelength laser bundle, and other wavelength laser or spectral signal are all had through characteristic.
8. according to arbitrary described laser probe analytical instrument in the claim 1 to 5, it is characterized in that the glass material of laser focusing objective len (17) is the ultraviolet fused quartz, glass surface is coated with anti-reflection film.
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